CN110590394A - Low-cost preparation method of large-size SiC nanowire aerogel - Google Patents
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Abstract
The invention discloses a low-cost preparation method of a large-size SiC nanowire aerogel, which comprises the steps of taking green and cheap starch as a carbon source, taking metal silicon as a silicon source, taking water as a solvent, adding a proper amount of foaming agent, carrying out sol, foaming, gel curing, carbonization and in-situ reaction to generate SiC nanowires, and interweaving and interconnecting the nanowires to obtain the SiC nanowire aerogel. After starch is dissolved in water to form sol, a large-size and high-porosity porous carbon blank is formed after gel curing and carbonization, a carbon source is provided for silicon-carbon reaction, and a space and a template are provided for SiC nanowire growth; with the progress of silicon-carbon reaction, the carbon net is continuously consumed, and simultaneously, SiC nanowires are generated in large quantity and are mutually crosslinked to obtain the large-size SiC nanowire aerogel. The method not only greatly reduces the manufacturing cost, but also solves the technical problem that the aerogel is difficult to prepare large-size products, and promotes the application of the SiC nanowire aerogel in the industrial fields of heat insulation, catalysis, filtration and the like.
Description
Technical Field
The invention belongs to the field of novel inorganic nano porous materials, and particularly relates to a low-cost preparation method of a large-size SiC nanowire aerogel.
Background
The aerogel is a nano-scale mesoporous composite material with low density, large specific surface area, high porosity and low heat conductivity coefficient, and has great application potential in the fields of high-temperature heat insulation systems, catalyst carriers, filters, electronics, optics and the like. However, the conventional ceramic aerogel is generally composed of nanoparticles, has low strength and high brittleness, is difficult to be manufactured into a large-sized product, and undergoes volume shrinkage at high temperature. Therefore, practical applications thereof have been limited. The SiC nanowire aerogel is a novel aerogel material, not only has the characteristics of ultralight, heat insulation, high specific surface area, strong adsorption and the like of the aerogel, but also has the performances of high temperature resistance, oxidation resistance, corrosion resistance, high strength, high elasticity, strong field emission and the like of the SiC nanowire, and particularly makes up for the defect of large brittleness of the traditional aerogel.
The document 'Ultralight, Recoverable, and High-Temperature-Resistant SiC Nanowire Aerogel' takes siloxane xerogel as a main raw material, and utilizes the in-situ growth and self-assembly technology of silicon carbide nanowires to prepare the ultra-light, High-elasticity, High-Temperature-Resistant and area larger than 150 cm2Nanowire aerogel paper with a density of only 5mg/cm3The porosity is as high as 99.8%. The patent No. 201810086069.9, SiC nanometer prepared by normal pressure CVD method with polycarbosilane as main raw materialThe line aerogel has small density, high purity and good light transmission. The SiC nanowire aerogel is a relatively new material, most of the SiC nanowire aerogel takes an organic ceramic precursor which is expensive and environmentally unfriendly as a raw material, and almost no research report about large-size products is reported, so that the industrial application of the material is greatly limited.
Disclosure of Invention
In order to solve the technical problems, the invention aims to provide a low-cost preparation method of a large-size SiC nanowire aerogel.
The technical scheme adopted by the invention for solving the technical problems is as follows:
a low-cost preparation method of a large-size SiC nanowire aerogel is characterized in that starch is used as a carbon source, metal silicon is used as a silicon source, water is used as a solvent, a dispersing agent and a foaming agent are added, and porous carbon is formed after sol, foaming, gel curing and carbonization of the starch; the porous carbon provides a growth space and a template for silicon-carbon reaction to generate SiC nanowires, the carbon structure is consumed along with the reaction, the SiC nanowires are generated in large quantity and are interwoven and interconnected to form macroscopic three-dimensional SiC nanowire aerogel, and the method comprises the following specific steps:
1) preparing a silicon-containing starch sol:
putting starch, metal silicon powder, water and a dispersing agent into a planetary ball mill according to a certain proportion, and performing ball milling and uniform mixing to obtain stable silicon-containing starch sol;
2) a foaming step:
adding a foaming agent into the silicaceous starch sol obtained in the step 1), stirring for 20min by using a stirrer, and standing for 2h at the temperature of 30 ~ 45 ℃ to obtain porous sol;
3) and (3) gel curing:
heating the porous sol obtained in the step 2) in a water bath at 80 ~ 100 ℃, preserving the heat for 40 min at 100 ℃, and drying the porous sol at 110 ℃ to constant weight to obtain porous gel;
4) and (3) carbonizing:
carbonizing the porous gel obtained in the step 3) to constant weight at 600 ℃ under the protection of nitrogen or argon to obtain a porous carbon sample.
5) Silicon-carbon reaction step:
and (3) under the protection of argon, heating the porous carbon sample obtained in the step (4) to 1350 ~ 1650 ℃ at the heating rate of 10 ~ 15 ℃/min, preserving the heat of 1350 ~ 1650 ℃ at 1650 ℃ for 3 ~ 10 h, cooling along with the furnace, and removing excessive carbon in air at 550 ℃ to obtain the SiC nanowire aerogel.
The starch in the step 1) is one or more of wheat starch, corn starch, sweet potato starch, sorghum starch and the like;
the dispersant in the step 1) is one or more of polyacrylamide, CAMTMENT FS20 and tetramethylethylenediamine.
The foaming agent in the step 2) is one or more of lauryl triethanolamine sulfate, yeast, egg white, baking soda and the like.
The mass ratio of the starch, the metal silicon powder, the foaming agent, the water and the dispersing agent in the steps 1) and 2) is 100: 5 ~ 20: 0.5 ~ 10:80 ~ 130:0.02 ~ 1.
The low-cost preparation method of the large-size SiC nanowire aerogel, provided by the invention, has the following characteristics by adopting the technical scheme:
1. the method takes starch and metal silicon as a carbon source and a silicon source, the raw materials are low in price, no toxic or harmful gas is emitted in the preparation process, and the method is green and environment-friendly;
2. in the preparation process, firstly, starch, silicon and water are prepared into silicon-containing starch sol, a large-size and high-porosity porous carbon template is obtained through foaming, gel curing and carbonization, then the carbon template is consumed through Si and C reaction, a large amount of SiC nanowires are generated, and the nanowires are mutually interwoven and interconnected to obtain the three-dimensional large-size SiC nanowire aerogel. The process is simple to operate, does not need supercritical drying, has low requirement on equipment and has strong safety;
3. the SiC nanowires obtained by the method through silicon-carbon in-situ reaction have high purity and small diameter (< 100 nm) and large length (>100 mu m), and the SiC aerogel formed by interweaving and interconnecting the nanowires has low density, large specific surface area, good toughness, moderate strength, excellent high-temperature stability and heat-insulating property, and wide application prospect in the industrial fields of heat insulation, catalysis, filtration and the like.
Drawings
Fig. 1 is a phase analysis XRD spectrum of the SiC nanowire aerogel prepared in example 1 of the method of the present invention.
Fig. 2 is a digital photograph of the SiC nanowire aerogel prepared in example 1 of the method of the present invention.
Fig. 3 is a scanning electron micrograph of the SiC nanowire aerogel prepared in example 1 of the method of the present invention (scanning electron micrograph of nanowire aerogel magnified 200 times).
Fig. 4 is a scanning electron micrograph of the SiC nanowire aerogel prepared in example 1 of the method of the present invention (field emission scanning electron micrograph of nanowire aerogel magnified 50000 times).
Detailed description of the preferred embodiments
The invention is described with reference to the accompanying drawings and specific examples:
example 1: putting 100 parts of wheat starch, 10 parts of metal silicon powder, 105 parts of water and 0.5 part of polyacrylamide into a planetary ball mill, and ball-milling for 2 hours at the speed of 30 r/min to obtain a silicon-containing starch sol; adding 1 part of yeast into the sol, stirring for 20min at the speed of 800 r/min, and preserving heat for 2h at 35 ℃ to obtain porous sol; putting the porous sol into a water bath, keeping the temperature at 100 ℃ for 40 min, taking out a sample, putting the sample into an oven, and drying the sample at 110 ℃ to constant weight to obtain porous gel; keeping the temperature of 600 ℃ in a nitrogen atmosphere until the weight is constant to obtain porous carbon; under the protection of argon, heating to 1350 ℃ at a heating rate of 15 ℃/min, preserving heat for 10 h, cooling along with a furnace, discharging carbon in air at 550 ℃ to constant weight to obtain the SiC nanowire aerogel, wherein a phase analysis XRD (X-ray diffraction) spectrum of the prepared SiC nanowire aerogel is shown in figure 1, a digital photo of the prepared SiC nanowire aerogel is shown in figure 2, a scanning electron microscope photo of the nanowire aerogel amplified by 200 times is shown in figure 3, and a field emission scanning electron microscope photo of the nanowire aerogel amplified by 50000 times is shown in figure 4.
Example 2: putting 100 parts of sorghum starch, 8 parts of metal silicon powder, 90 parts of water and 0.1 part of tetramethylethylenediamine into a planetary ball mill for ball milling for 2 hours at a speed of 30 r/min to obtain a silicon-containing starch sol; adding 1 part of yeast into the sol, stirring for 20min at the speed of 800 r/min, and preserving heat for 2h at 35 ℃ to obtain porous sol; putting the porous sol into a water bath, keeping the temperature at 95 ℃ for 40 min, taking out a sample, putting the sample into an oven, and drying the sample at 110 ℃ to constant weight to obtain porous gel; keeping the temperature at 600 ℃ in a nitrogen atmosphere until the weight is constant to obtain porous carbon; and under the protection of argon, heating to 1410 ℃ at the heating rate of 14 ℃/min, preserving the temperature for 4 h, cooling along with the furnace, and discharging carbon in air at 550 ℃ to constant weight to obtain the SiC nanowire aerogel.
Example 3: putting 100 parts of corn starch, 9 parts of metal silicon powder, 85 parts of water and 0.05 part of CAMTMENT FS20 into a planetary ball mill, and ball-milling for 2 hours at the speed of 30 r/min to obtain a silicon-containing starch sol; adding 1 part of yeast and 3 parts of baking soda into the sol, stirring at 800 r/min for 20min, and keeping the temperature at 35 ℃ for 2h to obtain porous sol; putting the porous sol into a water bath, preserving the heat at 98 ℃ for 40 min, taking out a sample, putting the sample into an oven, and drying the sample at 110 ℃ to constant weight to obtain porous gel; keeping the temperature at 600 ℃ in a nitrogen atmosphere to obtain porous carbon with constant weight; and under the protection of argon, heating to 1420 ℃ at the heating rate of 12 ℃/min, preserving heat for 2h, cooling along with the furnace, and discharging carbon in air at 550 ℃ to constant weight to obtain the SiC nanowire aerogel.
Example 4: putting 100 parts of wheat starch, 10 parts of metal silicon powder, 110 parts of water and 0.5 part of polyacrylamide into a planetary ball mill, and ball-milling for 2 hours at the speed of 30 r/min to obtain a silicon-containing starch sol; adding 5 parts of dodecyl sulfuric acid triethanolamine into the sol, stirring for 20min at the speed of 800 r/min, and keeping the temperature at 35 ℃ for 2h to obtain porous sol; putting the porous sol into a water bath, preserving the heat at 100 ℃ for 40 min, taking out a sample, putting the sample into an oven, and drying the sample at 110 ℃ to constant weight to obtain porous gel; keeping the temperature of 600 ℃ in a nitrogen atmosphere and balancing the weight to obtain porous carbon; under the protection of argon, the temperature is raised to 1350 ℃ at the heating rate of 10 ℃/min, the temperature is preserved at 1350 ℃ for 10 h, then the SiC nanowire aerogel is cooled along with the furnace, and carbon is discharged to constant weight in air at 550 ℃ to obtain the SiC nanowire aerogel.
Example 5, 100 parts of sorghum starch, 8 parts of metal silicon powder, 90 parts of water and 0.05 part of CAMTMENT FS20 are put into a planetary ball mill and ball milled for 2 hours at a speed of 30 r/min to obtain a silicon-containing starch sol, 5 parts of lauryl triethanolamine sulfate and 5 parts of 800 r/min are added into the sol and stirred for 10 minutes, heat preservation is carried out at a temperature of 25 ℃ for 2 hours to obtain porous sol, the porous sol is put into a water bath kettle and is subjected to heat preservation at a temperature of 94 ℃ for 40 minutes and drying at a temperature of 110 ℃ to constant weight to obtain porous gel, heat preservation and weight balancing are carried out at a temperature of 600 ℃ in a nitrogen atmosphere to obtain porous carbon, under the protection of argon, the temperature is increased to 1610 ℃ at a heating rate of 10 ~ 15 ℃/min, the temperature is preserved for 0.5 hours, furnace cooling is carried.
Claims (5)
1. A low-cost preparation method of a large-size SiC nanowire aerogel is characterized by comprising the following steps: according to the preparation scheme, starch is used as a carbon source, metal silicon is used as a silicon source, water is used as a solvent, a dispersing agent and a foaming agent are added, and porous carbon is formed after starch is subjected to sol, foaming, gel curing and carbonization; the porous carbon provides a growth space and a template for silicon-carbon reaction to generate SiC nanowires, the carbon structure is consumed along with the reaction, the SiC nanowires are generated in large quantity and are interwoven and interconnected to form macroscopic three-dimensional SiC nanowire aerogel, and the method comprises the following specific steps:
1) preparing a silicon-containing starch sol:
putting starch, metal silicon powder, water and a dispersing agent into a planetary ball mill according to a certain proportion, and performing ball milling and uniform mixing to obtain stable silicon-containing starch sol;
2) a foaming step:
adding a foaming agent into the silicaceous starch sol obtained in the step 1), stirring for 20min by using a stirrer, and standing for 2h at the temperature of 30 ~ 45 ℃ to obtain porous sol;
3) and (3) gel curing:
heating the porous sol obtained in the step 2) in a water bath at 80 ~ 100 ℃, preserving the heat for 40 min at 100 ℃, and drying the porous sol at 110 ℃ to constant weight to obtain porous gel;
4) and (3) carbonizing:
carbonizing the porous gel obtained in the step 3) to constant weight at 600 ℃ under the protection of nitrogen or argon to obtain a porous carbon sample.
5) Silicon-carbon reaction step:
and (3) under the protection of argon, heating the porous carbon sample obtained in the step (4) to 1350 ~ 1650 ℃ at the heating rate of 10 ~ 15 ℃/min, preserving the heat of 1350 ~ 1650 ℃ at 1650 ℃ for 3 ~ 10 h, cooling along with the furnace, and removing excessive carbon in air at 550 ℃ to obtain the SiC nanowire aerogel.
2. The low-cost preparation method of the large-size SiC nanowire aerogel as claimed in claim 1, wherein the preparation method comprises the following steps: the starch in the step 1) is one or more of wheat starch, corn starch, sweet potato starch, sorghum starch and the like.
3. The low-cost preparation method of the large-size SiC nanowire aerogel as claimed in claim 1, wherein the preparation method comprises the following steps: the dispersant in the step 1) is one or more of polyacrylamide, CAMTMENT FS20 and tetramethylethylenediamine.
4. The low-cost preparation method of the large-size SiC nanowire aerogel as claimed in claim 1, wherein the preparation method comprises the following steps: the foaming agent in the step 2) is one or more of lauryl triethanolamine sulfate, yeast, egg white, baking soda and the like.
5. The method for preparing the large-size SiC nanowire aerogel at low cost according to claim 1, wherein the mass ratio of the starch, the metal silicon powder, the foaming agent, the water and the dispersing agent in the steps 1) and 2) is 100: 5 ~ 20: 0.5 ~ 10:80 ~ 130:0.02 ~ 1.
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CN112457034A (en) * | 2020-11-10 | 2021-03-09 | 中钢南京环境工程技术研究院有限公司 | Preparation method of C/SiC composite material with vibrissa-nostril-like structure |
CN112736237A (en) * | 2021-01-19 | 2021-04-30 | 贵州大学 | Preparation method of green low-cost silicon-carbon anode material with three-dimensional porous structure |
CN113754462A (en) * | 2021-08-30 | 2021-12-07 | 常州大学 | Preparation of ultralight Cr capable of being rapidly cooled2O3-Al2O3Method for producing ceramic aerogels |
CN114349537A (en) * | 2022-01-25 | 2022-04-15 | 西安交通大学 | Super-elastic aerogel and preparation method thereof |
CN114715895A (en) * | 2022-04-14 | 2022-07-08 | 中国科学技术大学先进技术研究院 | Preparation method for elastic high-temperature-resistant silicon carbide aerogel based on melamine foam template structure |
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CN112457034A (en) * | 2020-11-10 | 2021-03-09 | 中钢南京环境工程技术研究院有限公司 | Preparation method of C/SiC composite material with vibrissa-nostril-like structure |
CN112736237A (en) * | 2021-01-19 | 2021-04-30 | 贵州大学 | Preparation method of green low-cost silicon-carbon anode material with three-dimensional porous structure |
CN112736237B (en) * | 2021-01-19 | 2023-05-02 | 贵州大学 | Preparation method of green low-cost silicon-carbon anode material with three-dimensional porous structure |
CN113754462A (en) * | 2021-08-30 | 2021-12-07 | 常州大学 | Preparation of ultralight Cr capable of being rapidly cooled2O3-Al2O3Method for producing ceramic aerogels |
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CN115246646A (en) * | 2021-12-22 | 2022-10-28 | 浙江理工大学 | Method for preparing silicon carbide nano-wire by using renewable resources or wastes as carbon source |
CN115246646B (en) * | 2021-12-22 | 2023-12-29 | 浙江理工大学 | Method for preparing silicon carbide nanowires by using renewable resources or wastes as carbon |
CN114349537A (en) * | 2022-01-25 | 2022-04-15 | 西安交通大学 | Super-elastic aerogel and preparation method thereof |
CN114715895A (en) * | 2022-04-14 | 2022-07-08 | 中国科学技术大学先进技术研究院 | Preparation method for elastic high-temperature-resistant silicon carbide aerogel based on melamine foam template structure |
CN114715895B (en) * | 2022-04-14 | 2023-09-05 | 中国科学技术大学先进技术研究院 | Preparation method of elastic high-temperature-resistant silicon carbide aerogel based on melamine foam template structure |
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